Allied Chemical Corporation

Allied Corporation

Alliedsignal Inc.

Emery J Carlson

John N Armor

Wim J Pieters

William E Gates

Jean Yamanis

Addison Miles Smith

William J Cunningham

John E Wilkalis

Guido P Pez

William C Conner, Jr

Chromium(III) oxide and hydroxide aerogels are produced by the reaction of chromium(VI) oxide with a solvent which is reducing to chromium(VI), such as methanol, heating the solution to hypercritical conditions, and venting the solvent hypercritically. The product aerogels exhibit surface areas above 400 m.sup.2 /g, pore volumes of at least 2 cm.sup.3 /g and a substantially uniform pore size distribution. Also disclosed is a unique process which employs high pore volume, high surface area chromium(III) oxide or hydroxide as a fluorination catalyst. More particularly, reaction of C.sub.2 Cl.sub.3 F.sub.3 with HF over these catalysts produced high yields of C.sub.2 Cl.sub.2 F.sub.4 and C.sub.2 ClF.sub.5.

Chromia aerogel, method of producing same and fluorination process

Chromium aerogel method of producing same and fluorinating process

A widely applicable and simple technique has been discovered for preparing aerogels in more durable forms. By the exposure of a variety of support structures to a pregel heated to hypercritical conditions, the resulting aerogel is produced and retained on the supporting structure. Thus, the aerogels are prepared and 'pelletized' in one step.

Production of aerogels on a support

Improved processes for the conversion to oximes by selective oxidation, in the vapor phase, of saturated primary aliphatic or alicyclic amines having 2 to 12 carbon atoms especially cyclohexylamine to cyclohexanone oxime with elemental oxygen, in a reaction zone, in the presence of an effective amount of a catalyst comprising an oxygen-containing tungsten compound and alumina by (1) periodically regenerating the oxygen-containing tungsten catalyst by heating same at about 250.degree. C.-300.degree. C. in the presence of elemental oxygen, or (2) maintaining the temperature of the oxygen-containing tungsten catalyst in a range of about 100.degree. C.-145.degree. C. or (3) employing higher mol fractions of oxygen and of amine in a range of about 0.2-0.4 in the vapor phase are disclosed. An improved method of preparing an oxygen-containing tungsten on an alumina catalyst is also disclosed.

Catalyst and method of making same for oxidation of primary amines to

A process is disclosed for the preparation of metallic products from metal salts admixed with solvent wherein at least one of the metal salt and the solvent is easily reducible. The admixture is heated under hypercritical conditions of temperature and pressure to produce metallic products and a hypercritical fluid. The hypercritical fluid is subsequently removed from the reaction zone and the metallic product is collected. The metallic product includes pure metals selected from the group of silver, gold, platinum, palladium, ruthenium, rhodium, mercury, arsenic, rhenium, tellurium, iridium, osmium, and copper, and alloys and mixtures thereof. The metallic product ordinarily exists as finely divided powders which may be highly porous.

Preparation of metal powders

Oxidation of primary amines to oximes by elemental oxygen with catalyst

A catalyst composition comprising a uniform dispersion of individual metallic palladium particles, substantially free of clusters of said particles, on and throughout an alumina aerogel support, said composition having a BET surface area in the range of about 20 to about 700 m.sup.2 /g, a pore volume in the range of about 1.5 to about 12 cm.sup.3 /g, a bulk density in the range of about 0.003 to about 0.5 g/cm.sup.3 and having a Pd.degree./Al.sub.2 O.sub.3 weight ratio of about 1:1000 to about 1:5 is disclosed. A process of preparing the catalyst composition having metallic palladium impregnated on alumina aerogel and a process of using same as a hydrogenation catalyst are also disclosed.

Palladium on alumina aerogel catalyst composition and process for making

An amorphous silica/alumina gel catalyst obtained by coprecipitating orthosilicate tetraester and aluminate triester in about 2.5:1 mole ratio, via rapid addition of about 0.4 to 5 moles of water per molecular equivalent of total ester groups, and drying at not over about 275.degree. C. is an effective catalyst for vapor phase reaction of cyclohexanone, ammonia and oxygen to form cyclohexanone oxime. This oxime can be rearranged to caprolactam, the starting material for nylon-6.

Process for ammoximation of cyclohexanone

Catalyst and process for the production of chlorofluorinated hydrocarbons are disclosed by reacting a hydrocarbon with HCl, HF and an oxygen-containing gas under oxychlorofluorination conditions in the presence of a catalytic composition comprising magnesium and copper ions each in combination with fluoride ions and an alkali metal ion, or mixtures thereof, in combination with chloride ions.

Catalyst and process for the production of chlorofluorinated hydrocarbons

Catalyst of cuprous chloride, as a first layer, on a carrier of particles of pyrogenic anhydrous silica or titania, or alpha-alumina produced from pyrogenic gamma-alumina, having as a second layer an alkali metal chloride especially KCl, and preferably also a rare earth metal chloride; especially LaCl.sub.3 ; formed by impregnation using non-aqueous solvents, especially CuCl in acetonitrile followed by KCl/LaCl.sub.3 in formic acid. The catalyst is effective at desirable reaction rates at temperatures well below 400.degree. C., such as 200.degree.-300.degree. C. and even below 200.degree. C., under certain conditions, for oxyhydrochlorination of organic materials such as methane; and is also effective for production of chlorine by the Deacon process at relatively low temperatures. Problems due to catalyst volatility and melting are substantially mitigated.

Pyrogenic silica or titania or alpha-alumina cuprous chloride catalyst

The catalyst consists essentially of a calcium fluoride matrix and a thermally stable copper-containing phase as produced by coprecipitation of calcium fluoride and copper fluoride and/or calcium hydroxide and copper oxide, in presence of alkali metal or ammonium ion. The coprecipitate is thoroughly dried and heated at elevated temperature; followed, if the coprecipitate is in the form of hydroxide and/or oxide, by conversion of such hydroxide and oxide to fluoride. The preferred alkali metal ion is potassium. The most active and stable catalysts show by X-ray diffraction a pattern including lines characteristic of calcium fluoride and additional lines indicative of a face-centered cubic unit cell having unit dimension of about 8.1-8.4 A. The catalyst operates at about 200.degree.-550.degree. C. depending to some extent on the substrate.

Catalyst of chlorination and combined chlorination/fluorination based on

Catalyst and process for the production of chlorofluorinated hydrocarbons are disclosed by reacting a hydrocarbon with HCl, HF and oxygen-containing gas under oxychlorofluorination conditions in the presence of a catalytic composition comprising magnesium and copper ions each in combination with fluoride ions and an alkali metal ion, or mixtures thereof, in combination with chloride ions.

A catalyst consisting essentially of cuprous chloride intercalated in crystalline boron nitride, containing at least 10% copper, useful for substitution chlorination of organic substances in vapor phase at elevated temperature by action of chlorine or HCL and oxygen. Highly selective for chlorination versus oxidation and hydrolysis even at high conversions, using partially chlorinated organic material as reactant, in particular methyl chloride.

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Chatham, NJ, United States of America

Emery J Carlson